CN116477970A - Preparation method of CMAS corrosion-resistant in-situ generated rare earth apatite phase compact reaction layer - Google Patents
Preparation method of CMAS corrosion-resistant in-situ generated rare earth apatite phase compact reaction layer Download PDFInfo
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- 230000007797 corrosion Effects 0.000 title claims abstract description 101
- 238000005260 corrosion Methods 0.000 title claims abstract description 101
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 91
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 78
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 76
- 229910052586 apatite Inorganic materials 0.000 title claims abstract description 74
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 title claims abstract description 74
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 239000011248 coating agent Substances 0.000 claims abstract description 79
- 238000000576 coating method Methods 0.000 claims abstract description 79
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 36
- 239000012720 thermal barrier coating Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000007747 plating Methods 0.000 claims abstract description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 10
- 238000007751 thermal spraying Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 55
- 239000011521 glass Substances 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000000498 ball milling Methods 0.000 claims description 19
- 238000005524 ceramic coating Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- 238000007750 plasma spraying Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 238000013461 design Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 6
- 238000005488 sandblasting Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000000080 wetting agent Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 5
- 238000012937 correction Methods 0.000 claims description 3
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 2
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000280 densification Methods 0.000 claims 1
- 238000002844 melting Methods 0.000 abstract description 8
- 230000008018 melting Effects 0.000 abstract description 8
- 230000008595 infiltration Effects 0.000 abstract description 7
- 238000001764 infiltration Methods 0.000 abstract description 7
- 229910000831 Steel Inorganic materials 0.000 abstract 1
- 239000006060 molten glass Substances 0.000 abstract 1
- 239000010959 steel Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 109
- 229910004283 SiO 4 Inorganic materials 0.000 description 24
- 238000002441 X-ray diffraction Methods 0.000 description 16
- 238000005530 etching Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 230000000149 penetrating effect Effects 0.000 description 5
- 230000035515 penetration Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 239000003822 epoxy resin Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 238000003837 high-temperature calcination Methods 0.000 description 4
- 229920000647 polyepoxide Polymers 0.000 description 4
- 239000011253 protective coating Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010952 in-situ formation Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- -1 rare earth cations Chemical class 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910010038 TiAl Inorganic materials 0.000 description 1
- 229910010041 TiAlC Inorganic materials 0.000 description 1
- 229910052661 anorthite Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000010987 cubic zirconia Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000000626 liquid-phase infiltration Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/89—Coating or impregnation for obtaining at least two superposed coatings having different compositions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/18—After-treatment
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/60—Efficient propulsion technologies, e.g. for aircraft
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- Plasma & Fusion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Structural Engineering (AREA)
- Coating By Spraying Or Casting (AREA)
Abstract
The invention discloses a preparation method of an in-situ generated rare earth apatite phase compact reaction layer for resisting CMAS corrosion, belonging to the field of Thermal Barrier Coating (TBCs) materials and preparation thereof. The invention adopts a plasma thermal spraying method to prepare a layer of rare earth oxide coating on the surface of a YSZ coating, and adopts a slurry brush plating method to coat a layer of uniform CaO-MgO-Al on the surface of the rare earth oxide coating 2 O 3 ‑SiO 2 After pre-corrosion treatment at 1250-1400 deg.c for 10-15min, thin and continuous compact reaction layer with excellent interface combination and comprising single high melting point rare earth apatite phase is produced on the surface of the coatingThe thickness of the steel plate after corrosion treatment at 1400 ℃ for 24 hours is not more than 9 mu m. The in-situ generated rare earth apatite phase compact reaction layer prepared by the method has good high-temperature thermochemical stability in high-temperature melting CMAS, effectively inhibits further infiltration corrosion of molten glass CMAS melt, and has excellent application prospect in the field of high-temperature protection.
Description
Technical Field
The invention relates to a rare earth oxide coating on the surface of a thermal barrier coating for resisting high-temperature corrosion of Huoshan gray CMAS glass, which is used for generating a rare earth apatite phase compact reaction layer in situ and a preparation method thereof, in particular to a rare earth apatite phase compact reaction layer for inhibiting molten CMAS infiltration corrosion and a preparation method thereof.
Background
As advanced aeroengines evolve to high thrust-to-weight ratios and high thermal efficiencies, the operating temperatures increase significantly. The inlet temperature of the front design of the first-stage aeroengine turbine with the new generation thrust weight ratio of 12-15 is over 2000K, and the environmental sediment (mainly CaO-MgO-Al) with the melting point of about 1240 ℃ is aggravated 2 O 3 -SiO 2 The CMAS) damages the penetration, dissolution and corrosion of the thermal barrier coating (Thermal barrier coatings, TBCs), so that the coating is subjected to phase change, heat conductivity, mechanical property and the like to deteriorate, stress, cracking and even peeling are generated, and the service performance and the safety and reliability of the engine are seriously affected. The TBCs working temperature is continuously increased, the environmental pollution is aggravated, the corrosion problem of CMAS on TBCs is increasingly outstanding, and the TBCs service working temperature and service life are limited. Corrosion protection is the focus of research in the TBCs field. For high temperature infiltration corrosion of CMAS glass, there is currently no viable material and technology worldwide. The protection strategy of TBCs in CMAS environment is a key for improving the development level of aeroengines.
The research shows that the high-melting-point rare earth apatite phase has excellent property of preventing the penetration and corrosion of the molten CMAS, and becomes a research hotspot and design basis of the CMAS barrier layer. Rare earth zirconate, silicate, phosphate and the like with high rare earth content (the rare earth content is up to 33% mol or more) can quickly react with molten CMAS under high temperature, dissolve out a large amount of rare earth cations, and react with Ca in CMAS melt 2+ And Si (Si) 4+ Affinity to form compact reaction layer of Ca-RE-Si apatite phase and anorthite and cubic zirconia with melting point of 1930 deg.c, and effective reactionThe reaction layer of the high temperature molten CMAS melt is inhibited. However, the compact reaction layer has multiple phases, which affects the mechanical property and deformation coordination of the compact reaction layer, and the thickness of the compact layer and the penetration depth of the melt are relatively large. The penetration depth was 20 μm at 1250℃and 100 μm or more at 1400 ℃. This requires a relatively large protective layer thickness on the TBCs surface, which affects the interfacial stress distribution and fatigue life of TBCs. The rare earth oxide coating designed by the invention generates a thin continuous compact reaction layer which is well combined in an interface and consists of a single high-melting-point rare earth apatite phase on the surface of the protective coating in situ after being pre-corroded by CMAS at a high temperature for a short time, has a thickness of 1-2 mu m, has good interface compatibility and mechanical property with a matrix protective coating, has excellent thermochemical stability in the molten CMAS, has a thickness of not more than 9 mu m after being reacted for 24 hours at 1400 ℃, has few molten CMAS permeated below the compact layer, shows excellent high-temperature-resistant molten CMAS permeation corrosion capability, and has excellent application prospects in the fields of thermal barrier coating materials and high-temperature protective coatings.
The prior protective coating material for resisting CMAS high temperature infiltration corrosion mainly comprises a non-wetting Pt layer, a non-wetting ceramic layer and LaP which are coated on the surface of TBCs 3 O 9 Coating, li 2 O-YSZ coating, high-entropy rare earth silicate, CMAS corrosion adhesion resistant thermal barrier coating, micro-nano double-scale structure corrosion resistant ceramic top layer, high-entropy ceramic material, rare earth zirconate coating and doped TiAl 3 RE3TaO7 coating, MAX phase TiAlC ceramic coating, and the like, with patent application numbers of CN108004543A, CN104988455A, CN102371734A, CN114671675A, CN108715988B, CN104988455B, CN114752881A, CN106086765B, CN112341197A, CN105862038A, CN113772723A, CN115074654A, CN111004990A, and the like, and relates to a ceramic coating material for resisting CMAS high-temperature corrosion and a preparation method thereof. The preparation method can be used for preparing the coating resisting the high-temperature corrosion of the molten CMAS.
The preparation process and the preparation method can prepare the high-temperature corrosion coating of CMAS glass, but the toughness of the coating is reduced due to complex components, or a plurality of coating layers, large thickness, a plurality of phases after reaction and the like, and the dissolution sacrificial layer has large infiltration, dissolution and corrosion thickness, poor interface bonding compatibility, large change and influence of stress fields on the surface of the coating and the like, so that the application performance is limited to a certain extent. Therefore, the development and preparation method and the operation are simple, the method is suitable for industrial production, and the method has the advantages of excellent thermochemical stability in high-temperature melting CMAS, effective inhibition of CMAS melt further infiltration corrosion, good in-situ growth of interface compatibility and important significance in a thin, continuous and compact high-melting-point rare earth apatite phase compact reaction layer.
Disclosure of Invention
The invention aims to improve and overcome the defects of the prior art, and provides a preparation method for an in-situ generated rare earth apatite phase compact reaction layer with thermochemical stability for resisting CMAS corrosion and high-melting-point interface combination. The preparation method has simple process and flow, the preparation technology with simple operation, high efficiency and controllable thickness is adopted, the in-situ generation of the rare earth apatite phase compact reaction layer is well combined with the matrix coating interface, the thickness is thin, the continuous compactness is realized, the composition phase is a single rare earth apatite phase, the thermochemical stability in high-temperature melting CMAS is good, and the high-temperature melting CMAS melt infiltration corrosion resistance is excellent.
The technical scheme of the invention is as follows: a preparation method of a compact reaction layer of an in-situ generated rare earth apatite phase for resisting CMAS corrosion comprises the following steps:
(1) Powder pretreatment: the rare earth oxide powder and the thermal barrier coating material powder are dried before being prepared into a ceramic coating by plasma spraying;
(2) Preparation of a ceramic coating: performing atmospheric plasma thermal spraying on the alumina thin plate subjected to polishing, sand blasting, ethanol ultrasonic cleaning and drying pretreatment to prepare a YSZ coating, and then performing plasma spraying deposition on the YSZ surface to deposit a rare earth oxide coating;
(3) Preparation of CMAS glass layer: coating a uniform CaO-MgO-Al layer on the surface of the rare earth oxide coating by adopting a slurry brush plating method 2 O 3 -SiO 2 (CMAS) glass layer;
(4) Preparation of a dense reaction layer of rare earth apatite phase: carrying out high-temperature short-time pre-corrosion treatment on the coating coated with the CMAS glass layer; after high temperature short time pre-corrosion treatment, a thin continuous compact reaction layer composed of rare earth apatite phase is generated on the surface of the coating in situ.
Preferably, the rare earth oxide powder in the step (1) is Gd 2 O 3 、La 2 O 3 、Y 2 O 3 、Yb 2 O 3 、Sm 2 O 3 、Dy 2 O 3 、Nd 2 O 3 、Er 2 O 3 、CeO 2 The powder is spherical powder with a particle size of 30-100 μm.
Preferably, the thickness of the plasma sprayed rare earth oxide coating in the step (2) is 10-20 μm.
Preferably, the CMAS glass in the step (3) is CaO-MgO-Al 2 O 3 -SiO 2 Glass with the components of 20-33CaO-8-10MgO-6-7Al 2 O 3 -45-58SiO 2 Glass (mole percent), caO, mgO, al 2 O 3 And SiO 2 Mixing the powder according to the corrected proportion to prepare materials, wherein the correction parameter is CaO 3-4% higher than the design amount, siO 2 The amount is reduced by 2-3% of the set amount, mgO and Al 2 O 3 Is unchanged.
Preferably, caO, mgO, al in the step (3) 2 O 3 And SiO 2 After powder is proportioned, ball milling is carried out, the parameters are 400-600r/min, the time is 4-6h, the wetting agent is ethanol, and the addition amount is 15%; drying and calcining at high temperature after ball milling to obtain massive transparent CMAS glass, wherein the temperature is 1350-1450 ℃ and the time is 3-4h; mechanically crushing, ball milling and sieving to obtain CMAS powder with granularity smaller than 200 mesh.
Preferably, the rare earth oxide coating surface in the step (3) is coated with a uniform CMAS glass layer, and the coating amount is 20-50mg/cm 2 。
Preferably, the pre-etching treatment temperature in the step (4) is 1250-1400 ℃ and the time is 10-15min.
Preferably, the pre-corrosion treatment in the step (4) is performed under the atmospheric environment, and the temperature rising speed is 5 ℃/min at the room temperature of between 1000 ℃ and 3 ℃/min at the temperature of between 1000 ℃ and 1400 ℃. And after the pre-corrosion treatment is finished, cooling along with the furnace, wherein the cooling speed is the same as the heating speed.
Preferably, after the pre-corrosion treatment in the step (4), a continuous compact reaction layer with the thickness of 1-2 mu m, which is formed by a single high-melting-point rare earth apatite phase and has good interface bonding, can be generated on the surface of the coating in situ.
Preferably, the continuous compact reaction layer of rare earth apatite obtained after the pre-corrosion treatment in the step (4) has good thermochemical stability in high-temperature molten CMAS, the thickness of the continuous compact reaction layer after the reaction at 1400 ℃ for 24 hours is not more than 9 mu m, the molten CMAS penetrating below the compact layer is very small, and the high-temperature molten CMAS melt penetration corrosion resistance is excellent.
Compared with the prior art, the preparation method for the in-situ generation of the rare earth apatite phase compact reaction layer has the following beneficial effects:
1. the process for preparing the in-situ generation rare earth apatite phase compact reaction layer is simple.
2. The in-situ generated rare earth apatite phase compact reaction layer is well combined with the interface of the matrix coating, and consists of a single-phase high-melting-point rare earth apatite phase.
3. The in-situ generated rare earth apatite phase compact reaction layer has high thermochemical stability in the molten CMAS, low growth speed and small thickness, and does not change the stress field of the coating.
4. The in-situ generated rare earth apatite phase compact reaction layer is continuous and compact, and has excellent performance of inhibiting high-temperature melting CMAS infiltration corrosion.
Drawings
FIG. 1 is a graph showing XRD of a sample of example 1 of the present invention, in which the prepared in-situ-formed dense reaction layer is a single rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites).
FIG. 1 is a XRD plot of a sample of example 2 of the present invention, wherein the in-situ-formed dense reaction layer is prepared as a single rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites).
Curve three of figure 1Is XRD curve of sample of example 3 of the invention, the prepared in-situ generated compact reaction layer is single rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites).
FIG. 1 is a graph showing XRD of sample 4 of the present invention, in which the prepared in-situ-formed dense reaction layer is a single rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites).
FIG. 2 is a graph showing XRD of sample 1 of the present invention, where a dense reaction layer was formed in situ after the pre-etching treatment, and remained as a single rare earth apatite phase (Ca after CMAS etching at 1250℃for 24 hours 4 Y 6 (SiO 4 ) 6 O, Y-apatites).
FIG. 2 is a XRD plot of sample 2 of the invention, where the pre-etch treatment was followed by in situ formation of a dense reaction layer, which remained as a single rare earth apatite phase (Ca after CMAS etching at 1400℃for 24 hours 4 Y 6 (SiO 4 ) 6 O, Y-apatites).
FIG. 2 is a plot III showing XRD of sample 3 of the invention, where the pre-etch treatment resulted in situ formation of a dense reaction layer, which remained as a single rare earth apatite phase (Ca after CMAS etch at 1250℃for 24 hours 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites).
FIG. 2 is a graph showing XRD of sample 4 of the present invention, where the dense reaction layer was formed in situ after the pre-etching treatment, and remained as a single rare earth apatite phase (Ca after CMAS etching at 1400℃for 24 hours 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites).
FIG. 3 is a cross-sectional profile of an in situ formed dense reaction layer prepared in example 1 of the present invention. The compact reaction layer is a single rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites) with a thickness of 0.8. Mu.m.
FIG. 4 is a cross-sectional profile of an in situ formed dense reaction layer prepared in example 1 of the present invention after CMAS corrosion at 1250℃for 24 hours. The compact reaction layer is singleRare earth apatite phase (Ca) 4 Y 6 (SiO 4 ) 6 O, Y-apatites) with a thickness of 1.9. Mu.m.
FIG. 5 is a cross-sectional profile of an in situ formed dense reaction layer prepared in example 2 of the present invention. The compact reaction layer is a single rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites) with a thickness of 1.7. Mu.m.
FIG. 6 is a cross-sectional profile of an in situ formed dense reaction layer prepared in example 2 of the present invention after CMAS corrosion at 1400℃for 24 hours. The compact reaction layer is a single rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites) with a thickness of 8.2. Mu.m.
FIG. 7 is a cross-sectional profile of an in situ formed dense reaction layer prepared in example 3 of the present invention. The compact reaction layer is a single rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites) with a thickness of 0.7 μm.
FIG. 8 is a cross-sectional profile of an in situ formed dense reaction layer prepared in example 3 of the present invention after CMAS corrosion at 1250℃for 24 hours. The compact reaction layer is a single rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 ) Composition, thickness 1.9 μm.
FIG. 9 is a cross-sectional profile of an in situ formed dense reaction layer prepared in example 4 of the present invention. The compact reaction layer is a single rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites) with a thickness of 1.9 μm.
FIG. 10 is a cross-sectional profile of an in situ formed dense reaction layer prepared in example 4 of the present invention after CMAS corrosion at 1400℃for 24 hours. The compact reaction layer is a single rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 ) Composition, thickness 9.0 μm.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A preparation method of an in-situ generated rare earth apatite phase compact reaction layer for resisting CMAS corrosion comprises the following steps:
(1) Powder pretreatment: to rare earth oxide Y 2 O 3 The powder and thermal barrier coating material powder (7-8% by weight yttria partially stabilized zirconia, YSZ) were baked prior to plasma spray preparation into a ceramic coating. The powder is spherical powder with particle diameter of 30-100 μm. The drying temperature is 120 ℃ and the drying time is 2 hours.
(2) Preparation of a ceramic coating: and performing atmospheric plasma thermal spraying on the alumina thin plate subjected to polishing, sand blasting, ethanol ultrasonic cleaning and drying pretreatment to prepare a YSZ coating, and then performing plasma spraying deposition on the YSZ surface to deposit a rare earth oxide coating.
The thickness of the YSZ coating is 100-120 mu m, and the thickness of the rare earth oxide coating on the surface of the YSZ coating is 15-20 mu m. The plasma spraying parameters are voltage 45V, current 700A, argon flow 1800L/h, hydrogen flow 200L/h, powder feeding speed 15g/min and spraying distance 120mm.
(3) Preparation of CMAS glass layer: coating a layer of uniform 33CaO-9MgO-13Al on the surface of the rare earth oxide coating by adopting a slurry brush plating method 2 O 3 -45SiO 2 (CMAS, mol%) glass layer.
1) 33CaO, 9MgO and 13Al 2 O 3 And 45SiO 2 (mol%) powder is mixed according to the corrected proportion and ball-milled, the corrected parameter is CaO ratio design amount higher than 3%, siO 2 The amount is reduced by 3 percent of the set amount, mgO and Al 2 O 3 Is unchanged. The ball milling parameter is 400r/min, the time is 6h, the wetting agent is ethanol, and the addition amount is 15%. And (3) performing drying and high-temperature calcination after ball milling to obtain the massive transparent CMAS glass, wherein the temperature is 1400 ℃ and the time is 4 hours. Mechanically crushing, ball milling and sieving to obtain CMAS powder with granularity smaller than 200 mesh.
2) Slurry brush plating CMAS layer: the CMAS powder slurry prepared by adopting proper amount of alcohol is coated with a uniform CMAS glass layer on the surface of the rare earth oxide coating, and the coating amount is 30mg/cm 2 。
(4) Preparation of a dense reaction layer of rare earth apatite phase: and carrying out high-temperature short-time pre-corrosion treatment on the coating after the CMAS glass layer is coated. The pre-corrosion treatment temperature is 1250 ℃ and the pre-corrosion treatment time is 15min. The pre-corrosion treatment is carried out in an atmospheric environment, the temperature rising speed is 5 ℃/min at the room temperature of-1000 ℃ and 3 ℃/min at the temperature of 1000-1250 ℃. And after the pre-corrosion treatment is finished, cooling along with the furnace, wherein the cooling speed is the same as the heating speed.
And (3) carrying out high-temperature CMAS long-time corrosion on the pretreated sample, wherein the temperature is 1250 ℃ and the time is 24 hours. The temperature rise and fall requirements are the same as above.
And (3) carrying out pre-corrosion treatment on the sample at 1250 ℃ for 15min, carrying out high-temperature CMAS (CMAS) on the pre-treated sample at 1250 ℃ for 24h, carrying out X-ray diffraction test analysis (XRD), cutting the sample, cold inlaying the epoxy resin, finely grinding and polishing, and observing the cross section morphology of the corroded ceramic coating by using a Scanning Electron Microscope (SEM). The test data obtained are shown in fig. 1 (curve one) and fig. 2 (curve one), and fig. 3 and fig. 4.
After 15min pre-corrosion at 1250 ℃, single high-melting-point rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites) of a continuous dense reaction layer having a thickness of 0.8. Mu.m. After CMAS etching at 1250 ℃ for 24 hours, the dense reaction layer formed by the pre-etching treatment is still a single rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites) to a thin and continuous dense reaction layer with a slow thickness growth of only 1.9 μm. The CMAS melt penetrating under the dense reaction layer was very small. The result shows that the rare earth apatite phase compact reaction layer formed by the pre-corrosion treatment is thin, continuous and compact, and has excellent thermochemical stability in the molten CMAS and CMAS high-temperature corrosion resistance.
Example 2
A preparation method of an in-situ generated rare earth apatite phase compact reaction layer for resisting CMAS corrosion comprises the following steps:
(1) Powder pretreatment: to rare earth oxide Y 2 O 3 The powder and thermal barrier coating material powder (7-8% by weight yttria partially stabilized zirconia, YSZ) were baked prior to plasma spray preparation into a ceramic coating.The powder is spherical powder with particle diameter of 30-100 μm. The drying temperature is 150 ℃ and the time is 1.5h.
(2) Preparation of a ceramic coating: and performing atmospheric plasma thermal spraying on the alumina thin plate subjected to polishing, sand blasting, ethanol ultrasonic cleaning and drying pretreatment to prepare a YSZ coating, and then performing plasma spraying deposition on the YSZ surface to deposit a rare earth oxide coating.
The thickness of the YSZ coating is 100-120 mu m, and the thickness of the rare earth oxide coating on the surface of the YSZ coating is 18-20 mu m. The plasma spraying parameters are 48V, 680A, 2000L/h argon flow, 220L/h hydrogen flow, 15g/min powder feeding speed and 150mm spraying distance.
(3) Preparation of CMAS glass layer: coating a layer of uniform 20CaO-9MgO-13Al on the surface of the rare earth oxide coating by adopting a slurry brush plating method 2 O 3 -58SiO 2 (CMAS, mol%) glass layer.
1) 20CaO, 9MgO and 13Al 2 O 3 And 58SiO 2 (mol%) powder is mixed according to the corrected proportion and ball-milled, the correction parameter is CaO ratio design quantity 3.5%, siO 2 The amount is reduced by 2.5% of the set amount, mgO and Al 2 O 3 Is unchanged. The ball milling parameter is 500r/min, the time is 5h, the wetting agent is ethanol, and the addition amount is 15%. And (3) performing drying and high-temperature calcination after ball milling to obtain the massive transparent CMAS glass, wherein the temperature is 1450 ℃ and the time is 3 hours. Mechanically crushing, ball milling and sieving to obtain CMAS powder with granularity smaller than 200 mesh.
2) Slurry brush plating CMAS layer: the CMAS powder slurry prepared by adopting proper amount of alcohol is coated with a uniform CMAS glass layer on the surface of the rare earth oxide coating, and the coating amount is 20mg/cm 2 。
(4) Preparation of a dense reaction layer of rare earth apatite phase: and carrying out high-temperature short-time pre-corrosion treatment on the coating after the CMAS glass layer is coated. The pre-corrosion treatment temperature is 1400 ℃ and the time is 10min. The pre-corrosion treatment is carried out in an atmospheric environment, the temperature rising speed is 5 ℃/min at the room temperature of-1000 ℃ and 3 ℃/min at the temperature of 1000 ℃ to 1400 ℃. And cooling the sample subjected to the high-temperature short-time pre-corrosion treatment to room temperature along with a furnace. The cooling speed is the same as the heating speed.
And (3) carrying out high-temperature CMAS long-time corrosion on the pretreated sample, wherein the temperature is 1400 ℃ and the time is 24 hours. The temperature rise and fall requirements are the same as above.
And (3) carrying out pre-corrosion treatment on the sample at 1400 ℃ for 10min, carrying out high-temperature CMAS long-time corrosion on the pre-treated sample at 1400 ℃ for 24h, adopting X-ray diffraction test analysis (XRD), cutting the sample, cold inlaying the epoxy resin, fine grinding and polishing, and observing the cross section morphology of the corroded ceramic coating by using a Scanning Electron Microscope (SEM). The test data obtained are shown in fig. 1 (curve two) and fig. 2 (curve two), and fig. 5 and fig. 6.
After pre-corrosion for 10min at 1400 ℃, single high-melting-point rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites) of a continuous dense reaction layer having a thickness of 1.7. Mu.m. After CMAS corrosion at 1400 ℃ for 24 hours, the dense reaction layer formed by the pre-corrosion treatment is still a single rare earth apatite phase (Ca 4 Y 6 (SiO 4 ) 6 O, Y-apatites) to a thin and continuous dense reaction layer with a slow thickness growth of only 8.2 μm. The CMAS melt penetrating under the dense reaction layer was very small. The result shows that the rare earth apatite phase compact reaction layer formed by the pre-corrosion treatment is thin, continuous and compact, and has excellent thermochemical stability in the molten CMAS and CMAS high-temperature corrosion resistance.
Example 3
A preparation method of an in-situ generated rare earth apatite phase compact reaction layer for resisting CMAS corrosion comprises the following steps:
(1) Powder pretreatment: to rare earth oxide Gd 2 O 3 The powder and thermal barrier coating material powder (7-8% by weight yttria partially stabilized zirconia, YSZ) were baked prior to plasma spray preparation into a ceramic coating. The powder is spherical powder with particle diameter of 30-100 μm. The drying temperature is 150 ℃ and the time is 1h.
(2) Preparation of a ceramic coating: and performing atmospheric plasma thermal spraying on the alumina thin plate subjected to polishing, sand blasting, ethanol ultrasonic cleaning and drying pretreatment to prepare a YSZ coating, and then performing plasma spraying deposition on the YSZ surface to deposit a rare earth oxide coating.
The thickness of the YSZ coating is 100-120 mu m, and rare earth oxide Gd on the surface of the YSZ coating 2 O 3 The thickness of the coating is 18-20 mu m. The plasma spraying parameters are 46V, 690A, 1800L/h of argon flow, 210L/h of hydrogen flow, 15g/min of powder feeding speed and 130mm of spraying distance.
(3) Preparation of CMAS glass layer: coating a layer of uniform 33CaO-9MgO-13Al on the surface of the rare earth oxide coating by adopting a slurry brush plating method 2 O 3 -45SiO 2 (CMAS, mol%) glass layer.
1) 33CaO, 9MgO and 13Al 2 O 3 And 45SiO 2 (mol%) powder is mixed according to the corrected proportion and ball-milled, the corrected parameter is CaO ratio design amount higher than 3%, siO 2 The amount is reduced by 3 percent of the set amount, mgO and Al 2 O 3 Is unchanged. The ball milling parameter is 400r/min, the time is 5.5h, the wetting agent is ethanol, and the addition amount is 15%. And (3) performing drying and high-temperature calcination after ball milling to obtain the massive transparent CMAS glass, wherein the temperature is 1450 ℃ and the time is 3.5h. Mechanically crushing, ball milling and sieving to obtain CMAS powder with granularity smaller than 200 mesh.
2) Slurry brush plating CMAS layer: the CMAS powder slurry prepared by adopting proper amount of alcohol is coated with a uniform CMAS glass layer on the surface of the rare earth oxide coating, and the coating amount is 25mg/cm 2 。
(4) Preparation of a dense reaction layer of rare earth apatite phase: and carrying out high-temperature short-time pre-corrosion treatment on the coating after the CMAS glass layer is coated. The pre-corrosion treatment temperature is 1250 ℃ and the pre-corrosion treatment time is 15min. The pre-corrosion treatment is carried out in an atmospheric environment, the temperature rising speed is 5 ℃/min at the room temperature of-1000 ℃ and 3 ℃/min at the temperature of 1000-1250 ℃. And after the pre-corrosion treatment is finished, cooling along with the furnace, wherein the cooling speed is the same as the heating speed.
And (3) carrying out high-temperature CMAS long-time corrosion on the pretreated sample, wherein the temperature is 1250 ℃ and the time is 24 hours. The temperature rise and fall requirements are the same as above.
And (3) carrying out pre-corrosion treatment on the sample at 1250 ℃ for 15min, carrying out high-temperature CMAS (CMAS) on the pre-treated sample at 1250 ℃ for 24h, carrying out X-ray diffraction test analysis (XRD), cutting the sample, cold inlaying the epoxy resin, finely grinding and polishing, and observing the cross section morphology of the corroded ceramic coating by using a Scanning Electron Microscope (SEM). The test data obtained are shown in fig. 1 (curve three) and fig. 2 (curve three), and fig. 7 and fig. 8.
After 15min pre-corrosion at 1250 ℃, single high-melting-point rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites) of 0.7 μm thick. After CMAS etching at 1250 ℃ for 24 hours, the dense reaction layer formed by the pre-etching treatment is still a single rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites) to a thin and continuous dense reaction layer, with a slow thickness growth of only 1.9 μm. The CMAS melt penetrating under the dense reaction layer was very small. The result shows that the rare earth apatite phase compact reaction layer formed by the pre-corrosion treatment is thin, continuous and compact, and has excellent thermochemical stability in the molten CMAS and CMAS high-temperature corrosion resistance.
Example 4
A preparation method of an in-situ generated rare earth apatite phase compact reaction layer for resisting CMAS corrosion comprises the following steps:
(1) Powder pretreatment: to rare earth oxide Gd 2 O 3 The powder and thermal barrier coating material powder (7-8% by weight yttria partially stabilized zirconia, YSZ) were baked prior to plasma spray preparation into a ceramic coating. The powder is spherical powder with particle diameter of 30-100 μm. The drying temperature is 150 ℃ and the time is 1.5h.
(2) Preparation of a ceramic coating: and performing atmospheric plasma thermal spraying on the alumina thin plate subjected to polishing, sand blasting, ethanol ultrasonic cleaning and drying pretreatment to prepare a YSZ coating, and then performing plasma spraying deposition on the YSZ surface to deposit a rare earth oxide coating.
The thickness of the YSZ coating is 100-120 mu m, and rare earth oxide Gd on the surface of the YSZ coating 2 O 3 The thickness of the coating is 16-20 mu m. The plasma spraying parameters are voltage 50V, current 650A and argon flow2100L/h, hydrogen flow 220L/h, powder feeding speed 18g/min and spraying distance 150mm.
(3) Preparation of CMAS glass layer: coating a layer of uniform 21CaO-9MgO-13Al on the surface of the rare earth oxide coating by adopting a slurry brush plating method 2 O 3 -57SiO 2 (CMAS, mol%) glass layer.
1) 20CaO, 9MgO and 13Al 2 O 3 And 58SiO 2 (mol%) powder is mixed according to the corrected proportion and ball-milled, the corrected parameter is CaO ratio design quantity is 4%, siO 2 The amount is reduced by 2% of the set amount, mgO and Al 2 O 3 Is unchanged. The ball milling parameter is 600r/min, the time is 4h, the wetting agent is ethanol, and the addition amount is 15%. And (3) performing drying and high-temperature calcination after ball milling to obtain the massive transparent CMAS glass, wherein the temperature is 1400 ℃ and the time is 4 hours. Mechanically crushing, ball milling and sieving to obtain CMAS powder with granularity smaller than 200 mesh.
2) Slurry brush plating CMAS layer: the CMAS powder slurry prepared by adopting proper amount of alcohol is coated with a uniform CMAS glass layer on the surface of the rare earth oxide coating, and the coating amount is 35mg/cm 2 。
(4) Preparation of a dense reaction layer of rare earth apatite phase: and carrying out high-temperature short-time pre-corrosion treatment on the coating after the CMAS glass layer is coated. The pre-corrosion treatment temperature is 1400 ℃ and the time is 10min. The pre-corrosion treatment is carried out in an atmospheric environment, the temperature rising speed is 5 ℃/min at the room temperature of-1000 ℃ and 3 ℃/min at the temperature of 1000 ℃ to 1400 ℃. And cooling the sample subjected to the high-temperature short-time pre-corrosion treatment to room temperature along with a furnace. The cooling speed is the same as the heating speed.
And (3) carrying out high-temperature CMAS long-time corrosion on the pretreated sample, wherein the temperature is 1400 ℃ and the time is 24 hours. The temperature rise and fall requirements are the same as above.
And (3) carrying out pre-corrosion treatment on the sample at 1400 ℃ for 10min, carrying out high-temperature CMAS long-time corrosion on the pre-treated sample at 1400 ℃ for 24h, adopting X-ray diffraction test analysis (XRD), cutting the sample, cold inlaying the epoxy resin, fine grinding and polishing, and observing the cross section morphology of the corroded ceramic coating by using a Scanning Electron Microscope (SEM). The test data obtained are shown in fig. 1 (curve four) and fig. 2 (curve four), and fig. 9 and fig. 10.
After pre-corrosion for 10min at 1400 ℃, single high-melting-point rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites) to a thickness of 2.0 μm. After CMAS corrosion at 1400 ℃ for 24 hours, the dense reaction layer formed by the pre-corrosion treatment is still a single rare earth apatite phase (Ca 2 Gd 8 (SiO 4 ) 6 O 2 Gd-apatites) to a thin and continuous dense reaction layer, with a slow thickness growth of only 9.0 μm. The CMAS melt penetrating under the dense reaction layer was very small. The result shows that the rare earth apatite phase compact reaction layer formed by the pre-corrosion treatment is thin, continuous and compact, and has excellent thermochemical stability in the molten CMAS and CMAS high-temperature corrosion resistance.
The above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or simple substitutions that do not undergo the inventive work should be covered in the scope of the present invention.
Claims (10)
1. The preparation method of the in-situ generated rare earth apatite phase compact reaction layer for resisting CMAS corrosion is characterized by comprising the following steps:
(1) Powder pretreatment: the rare earth oxide powder and the thermal barrier coating material powder are dried before being prepared into a ceramic coating by plasma spraying;
(2) Preparation of a ceramic coating: performing atmospheric plasma thermal spraying on the alumina thin plate subjected to polishing, sand blasting, ethanol ultrasonic cleaning and drying pretreatment to prepare a YSZ coating, and then performing plasma spraying deposition on the YSZ surface to deposit a rare earth oxide coating;
(3) Preparation of CMAS glass layer: coating a uniform CaO-MgO-Al layer on the surface of the rare earth oxide coating by adopting a slurry brush plating method 2 O 3 -SiO 2 A glass layer;
(4) Preparation of a dense reaction layer of rare earth apatite phase: carrying out high-temperature short-time pre-corrosion treatment on the coating coated with the CMAS glass layer; after the pre-corrosion treatment, a thin continuous compact reaction layer composed of rare earth apatite phases can be obtained on the surface of the coating in situ.
2. The method for preparing the compact reaction layer of the in-situ generated rare earth apatite phase for resisting CMAS corrosion according to claim 1, wherein the rare earth oxide powder in the step (1) is Gd 2 O 3 、La 2 O 3 、Y 2 O 3 、Yb 2 O 3 、Sm 2 O 3 、Dy 2 O 3 、Nd 2 O 3 、Er 2 O 3 、CeO 2 The thermal barrier coating material is 7-8% by weight yttria partially stabilized zirconia (YSZ); the powder is spherical powder with particle diameter of 30-100 μm.
3. The method for preparing the in-situ generated rare earth apatite phase compact reaction layer resistant to CMAS corrosion according to claim 2, wherein the drying temperature is 120-180 ℃ and the time is 1-2h.
4. The method for preparing an in-situ generated rare earth apatite phase densification reaction layer resistant to CMAS corrosion according to claim 3, wherein the YSZ coating in the step (2) has a thickness of 100-120 μm and the rare earth oxide coating on the surface of the YSZ coating has a thickness of 10-20 μm; the plasma spraying parameters are voltage 45-55V, current 600-750A, argon flow 1500-2300L/h, hydrogen flow 180-300L/h, powder feeding speed 10-20g/min and spraying distance 100-180mm.
5. The method for preparing a dense reaction layer of in-situ generated rare earth apatite phase for resisting CMAS corrosion according to claim 4, wherein the CMAS glass in the step (3) is CaO-MgO-Al 2 O 3 -SiO 2 Glass with components of 20-33 mol percent CaO-8-10MgO-6-7Al 2 O 3 -45-58SiO 2 Glass.
6. According to claimA process for preparing a dense reaction layer of in-situ generated rare-earth apatite phase for resisting CMAS corrosion as claimed in claim 5, wherein CaO, mgO, al is prepared by 2 O 3 And SiO 2 Mixing the powder according to the corrected proportion, performing ball milling, wherein the correction parameter is CaO 3-4% higher than the design amount, and SiO 2 The amount is reduced by 2-3% of the set amount, mgO and Al 2 O 3 The ball milling parameter is 400-600r/min, the time is 4-6h, and the wetting agent is 15% ethanol; drying and calcining at high temperature after ball milling to obtain massive transparent CMAS glass, wherein the temperature is 1350-1450 ℃ and the time is 3-4h; mechanically crushing, ball milling and sieving to obtain CMAS powder with granularity smaller than 200 mesh.
7. The preparation method of the CMAS corrosion resistant in-situ generated rare earth apatite phase compact reaction layer as claimed in claim 1 or 6, wherein the slurry brush plating method adopted in the step (3) is used for coating a uniform CMAS glass layer on the surface of the rare earth oxide coating, and the deposition amount is 20-50mg/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The CMAS slurry is prepared by dropping a proper amount of ethanol into the powder.
8. The method for preparing a dense reaction layer of rare earth apatite phase in situ generated against CMAS corrosion according to claim 7, wherein the pre-corrosion treatment temperature in step (4) is 1250-1400 ℃ and the time is 10-15min.
9. The method for preparing the in-situ generated rare earth apatite phase compact reaction layer resisting CMAS corrosion according to claim 8, wherein the pre-corrosion treatment is performed in an atmospheric environment, and the temperature rising speed is 5 ℃/min at the room temperature of between 1000 ℃ and 3 ℃/min at the temperature of between 1000 ℃ and 1400 ℃; and after the pre-corrosion treatment is finished, cooling along with the furnace, wherein the cooling speed is the same as the heating speed.
10. The method for preparing the compact reaction layer of the in-situ generated rare earth apatite phase for resisting CMAS corrosion according to claim 8, wherein the continuous compact reaction layer with the thickness of 1-2 μm, which is composed of a single high-melting-point rare earth apatite phase and has good interface bonding, can be obtained in-situ on the surface of the coating after the pre-corrosion treatment.
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